Sulphur-containing structure and method of making same



Patented Sept. 9, i924.

entre". srr

COMPANY, or BAY CITY, TEXAS, A CORPORATION OF TEXAS.

SULPHUR-CONTAINING STRUCTURE ANI) METHOD OF MAKING SAME.

Application led November 24, 1923. Serial No. 676,871.

To all whom z't may cof/wcm.'

Be it known thatfI, WILLIAM I-I. KOBB, a citizen'of the United States, residing at New York city, in the county of New York,

- State of New York, have invented certain new and useful Improvements in Sulphur- Containing Structures and Methods of Making Same; land I do hereby'declare the following to be a full, clear, and exact del scription of the invention, suchas will enable others skilled. in the art to which it ap- -pertains to make and use the same.

This invention relates to sulphur-'containing structures and methods of making'the llvsame. VThe invention has for its principal Object the provision of an improved method of making structures composed at least in part of an intimate mixture of sulphur and finely divided carbonaceous material. More `.20 particularly, the invention aims to provide an improved method ofimaking tanks or revceptacles for corrosive liquors composed in Whole or in part of a mixture of sulphur D and finely divided carbonaceous material. Further objects lof the invention will be discussed vin the course of the following description.

In my, copending patent applications, Serial No. 659,108, filed August 24:, 1923 and ,30 Serial No. 662,356 filed September 12, 1923,

I have described certain applications of a sulphur compound composed for the most art of an intimate mixture of sulphur and nnely divided carbonaceous material. Various forms of carbonaceous -material are available such, for example, as finely divided coke, anthracite coal, charcoal, carbon black, etc. Such a sulphur com ound effectively resists the action of aci s, alkalies, and

-many other corrosive liquors, an`d on this account such sulphur compounds are especially useful in the manufacture 4of tanks, receptacles, or the like, for containing corrosive liquors.

l At the presenttime, Wooden tanks are extensively used in many industries for holdingcorrosive liquors. Thus, wooden tanks are' used for vthe storage of acids, alkalies and other corrosive liquors and also for containing such corrosive liquors inthe course of some treatment process. For example, ,in metal-pickling it is customary to dip the metal int) an acid solntion, and the pickling solution isA generally contained in a i 55 Wooden tank. Considerable annoyance is Suchv sulphur compounds-are prepared by melting an appropriate quantity of sulphur andintimately incorporatingminthe molten WILLIAM HOFFMAN KOBB, OF NEW YO'RK, N. Y., ASSIGNOR TO TEXAS GULF SULPHUR V sulphur an appropriate quantity of the finely divided carbonaceous material. The resulting mixture is fluid and can be easily poured at temperatures .slightly above the melting temperature'of sulphur. Tanks or receptacles of small dimensions and similar objects and structures fcan be readily cast of such a sulphur compound. I have now found however that considerable difficulty is encountered in casting large masses of. such a sulphurcompound, due to internal stresses set up during solidification which result in cracks in the final structure.

In the course of my experiments and investigations, I have found that it is very difficult and substantially impossible under practical plant conditions to cast large masses of the aforementioned sulphur comand solidify in advance of otherA portions.

Thel sulphur compounds contract on cooling and solidifying and where the cooling and solidification are non-uniform throughout the mass, cracks almost inevitably result.

I have discovered that structures of large size can be satisfactorily made, in wholev or in part, of the aforementioned sulphur compounds, by introducing material into an appropriate form or mld and then filling -the voids or spaces between the individual lumps of the aggregate material with the sulphur compound in a molten condition. The sul-A phur compound is then allowed to solidify in situ in the voids within the mass of aggregate material and there results a monolithic structure of the desired size and configuration.

Any suitable aggregate material may be employed in carrying out the present invention. By aggregate material I mean material inthe form of lumps, generally irregular is size and configuration. In general, the

individual lumps may range in size from about one to about three inches, although 1t A will of course be understood that different' divided carbonaceous material. The aggre-A gate material may consist of crushedtrap rock, silicious rock, gravel, coke, scrap metal, and' the like.

In the single figure of the, accompanying drawing, I have diagrammatically repre-w sented the making of a metal-pickling tank in accordance with the principles of the present invention. l

.Referring to the drawing, the tank-is made on a concrete floor or foundation l. A rectangular enclosure 2 is first built upon the foundation l. This enclosure may convenientlybe made of two inch wooden planks and may be held together by tie-rods 3. I prefer, in some cases, to. build the enclosure 2 as a permanent outer covering or wall for the finished structure.

Within the enclosure 2 and appropriately spaced therefrom is erected a temporary rectangular structure 4. 'Ihe structure 4 may conveniently be made of one inch boards. The enclosures 2 and 4 constitute a form or mold and the spaces between these enclosures is filled with thel sulphur-containing ma- 'terial in accordance with the principles of the spaces between the enclosures 2 and 4 are gate material mayy conveniently be in the v first filled with aggregate material. In a tank of the dimensions mentioned this aggreform of lumps of from .l to '3 inches in size. The lumps of aggregate material will ordi` narily be of irregular configuration and there will exist within the mass o f aggregate material numerous spaces or voids. \'I`-heV aggregate material may consist of crushedrock,

" gravel, 4or other appropriate material. The

aggregate material need not necessarily beeinert with respect to the liquors used in the tank, since, as hereinafter explained, the inside or exposed surfaces of the tank are preferably v-covered with a thin layer of the corrosion-resisting sulphur compound. '-Where 1t is desiredto build the ent-ire tank .of the insediati corrosion-resisting sulphur compound, the aggregate' material `lmay consist of lumps of the compound itself. Thus, the sulphur compound may be solidified in Alarge blocks or cakes and subsequently crushed, and screened if4 necessary, to provide aggregate material of appropriate size.

'Ihe voids or spaces within the massk of aggregate lmaterial (confined between the enclosures 2 and 4) are nextiilled with the corrosion-resisting sulphur compound in a m'olten condition. To this end, an appropriate molten mixture of sulphur and finely divided carbonaceous material is made and is poured, upon the topof the mass of aggregate material. Preferably, the pouring of the molten sulphur compound takes place simultaneously at several points. The idea is to insure the penetration of the molten compound throughout the'entire mass of thel aggregate material. In a tank of thedimensions hereinbefore mentioned, 'satisfac- `compound should be slightly above the melting temperature of the sulphur, but should not be so high that the sulphur becomes viscous. In' other words, the sulphur compound at the time of pouring should be a freely-flowing liquid.

The sulphur compound is permitted to gregate material. There results a monolithic structure in whichthe .individual lumps of the aggregate material are firmly bonded or cemented together. By a monolithic structure, -I mean one in which the component parts thereof are firmly bonded together in the form of a unitary and substantially homogeneous mass. Where the aggregate material is composed of the corrosion-resistingsulphur compound, the monolithic structure wi be throughout a homogeneous mixture of ysulphur and finely divided carbonaceousmaterial.

When the four walls of t-he tank have been constructed as described, the inner enclosure 4 is removed. An .appropriate depth of gregate material .is =then spread upon the foundation 1 and within the enclosing walls 5y ofthe tank. Thereupon, the corrosion-redition is poured upon this aggregate material, preferably sin'iultaneously at a plu-l rality of points, and upon filling the voids in the aggregate material and soliditying in situ forms the bottom6 of the tank.

AThe inner or exposed surfaces of the tank are next preferably coated or covered with a t-hin layer 7 of the corrosion-resisting solidify in'situwithin the mass of the' agllO sulphur compound. In order' to avoid cracking of this surfacing layer I have found that it is necessary to apply the coating in thin films permitting partial solidication between successive applications of the films. This can be conveniently accomplished by applying the molten sulphur compound to the exposed surfaces With a brush or broom. In other- Words, the molten sulphur compound is painted or svvashed on to thevexposed surfacesin relatively thin films until a coating or vlayer of the desired thickness has been built up.-

The tops of the Walls 5 of the tank illustrated in the drawing are covered Withl planks 8.` -If desired, a Wooden frame 9 may be laid upon the bottom 6 of the tank and may be anchored-in position (so that it Will not float in the liquor in the tank) by Wooden blocks 10 secured to the top Wall planks 8.

The sulphur l compoundl whichy I ordi- `narily prefer to employis composedof about 60% sulphur andv 40%A of finely divided coke. Preferably, the coke is through QO mesh. It Will, of course, be

-understood that other finely divided carbonaceous materials may be employed and that the relative proportions of sulphur and 'carbonaceous material may be varied Without departing from the spirit of the present invention.

I have found the ordinary asphalt melter suitable for the preparation of the sulphur compound. A five barrel asphalt melter on` Wheels is a convenient size and type to employ. I prefer to use. a Hauck burner for heating the melter, since it is susceptible of convenient control. The heating of the sulphur compound must be carefully controlled after the sul-phur becomes melted, in order to avoid raising the temperature lof the molten mass to the. temperature at which sulphur becomes viscous. I have found that satisfactory results are secured by maintaining the molten mass in lthe melter at a temperature of from 125O C. to 150 C.

In preparing the sulphur compound, the carbonaceous material, such as coke, is first ground to a relatively fine powder. The sulphur is then melted and the temperature raised to slightly above the melting point,

say to about 12b-150o C. The finely divided carbonaceous material is then poured into the molten sulphur and intimately mixed. I prefer to add the'carbonaceous material in small instalments, say a shovelfull at a time, and to thoroughly agitateV or stir the molten mass, so as to insure com-v plete and uniform incorporation of the finely divided carbonaceous material.

The aggregate material is placed in the forms at atmospheric temperature. The mass of aggregate material is thus relatively cold compared with the molten sulphur compound subsequently poured thereon. I believe that this condition of the aggregate material, that is, 'beingrelatively cold, and its cooling capacity in consequence thereof contributes very largely to the making of these large tanks or receptacles Without'. cracking. As a result of this large bulk of relatively' cold material, the molten sulphur compound cools and solidifies more uniformly throughout the entire mass and there is consequently less pronouncedstrains Within the mass as a result of the contraction of the sulphur-compound during solidification. Uutlets and other appropriate-connections may be incorporated in the Walls of the tank during its formation; Thus, hollow tubes. of cardboard or the like, may be embedded inthe aggregate material and may form appropriate holes or outlets through the Wall of the tank when completed. When. the tank is composed throughout of the corrosion-resisting sulphur compound, holes may be made or bored in the' walls by means of a hot pipe or poker. If desired, iron.

ipes of relatively large 'diameter may be 9.0 filled With the sulphur compound and eme bedded'in the mass of aggregate material, and after the tank is completed a hole of smaller diameter may be bored or reamed thro-ughl the sulphur compound Within the -nent retention of the outer enclosing Wall 2 (in the accompanying dravving) is optional,

and thisv Wall, may, if desired, be removed y leaving the monolithic structure' standing 110 alone. If desired, Athe outer Wall of the structure may be banked up with dirt, clay-, i

or other appropriate mate-rial. Reinforcing agencies may also, if desired, be included in the aggregate material and thus incorporated in the completed structure.

A monolithic 4structure/made in accord-v ance with the present invention can be readily repared, incase of breaks or cracks therein, in accordance with the principles of the invention for making' the completed receptacle. Thus, the broken Lor cracked port-ion of the structure may be cut outv andl an appropriate. enclosure or form erected about the cut-out portion. This temporaryV `form is then filled With aggregate material and the voids therein filled with the compound of sulphur and finely divided carbonaceous material in a molten condition. Upon solidification ofthe sulphur compound, the repaired portion willbe found monolithically united with the remainder of the structure. 'Iclaim:- A j n 1. The method of making structures composed at least in part of a compound of in timately mixed sulphur and finely divided "'"carbonaceous 'material which comprises ap- Apropriately confining -a mass of aggregate material, filling the voids throughout the mass' of aggregate material with-the compound of intimately mixed sulphur and finely divided carbonaceous material in a molten condition, and permitting vsaid compound to solidify in situ whereby the ag gregate material and sulphur compound are bonded together to form av monolithic struc-- ture.

` f' 2.' The method of making structures oomposed at least in part of a compound of intimately -mixed sulphur and finely divided coke which comprises. appropriately confin ing a mass of aggregate material, filling the voids throughout the mass of aggregate material with the compound of" intimately mixed sulphur and-coke in a molten condi-- tion, and permitting said compoundto solidify in situ whereby the aggregate material and sulphur compound are bonded together to form a monolithic structure.

3. The method of making receptacles'l for corrosive liquors and the like which comprises appropriately confining a mass of aggregate material, filling the voids throughout the'massof aggregate material with a molten compound of intimately mixed sulphur and finely divided carbonaceous material, and permitting the -sulphur compound to solidify in situ in the mass of aggregate material whereby the aggregate material and sulphur compound are bonded together and Aform a monolithic structure.

4. The method of making receptacles for corrosive liquors and the like which comprises appropriately confining a massvof aggregate material, fillingthe voids throughout the mass of aggregate material with a.

- molten compound of intimately mixed sulphur and finely dividedlcoke, andAperm-itting the sulphur compound to solidify in situ in the mass of aggregate material whereby the aggregate material and sulphur compound are bonded together and form a monolithic structure.

` 5. lThe method ofymakingstructures composed at least in part of al compound of.

intimately mixed sulphur and finely divided carbonaceous material which'compri'ses in# troducing aggregate material latapproximately atmospheric temperature in to an appropriate form, filling theI voids Within the mass of the aggregate material with the compound of sulphur and finely divided car;

-bonaceous material in a molten condition, k and permitting said compound to solidfy in ,a thin layer of the sulphur compound to ioaiea 1 situ whereby the aggregate material and sulphurcompound form a monolithic structure.

6. The method of making structures composed at least invpart of a compound of intimately mixed sulphur and nely divided carbonaceous material which comprises introducing aggregate -material at approximately atmospheric temperature into an appropriate vform, filling the voids within the mass of the aggregate material with the compound of sulphur and finely divided carbonaceous material in a molten condition, permitting said compound to solidify in4 situ whereby the aggregate material and sulphur compound form a monolithic structure, and covering exposed surfaces of said structure with a relatively thin layer of said sulphur compound by the successive applioation to in molten condition and solidification on su'ch Isurfacesof films ofthe sulphur compound.

7,. The' method of making structures composed at least in part of a compound of intimately mixed sulphur and finely divided carbonaceous material which' comprises appropriately confining a mass of aggregate material, filling the voids throughout vthe mass of aggregate material with the comgregate material,filling the ,voids throughout the mass' of aggregate material with a molten compound of intimately mixed sulphur aid finely divided coke, permitting the sulphur compound to solidify in situ in the mass of aggregate material whereby the aggregate material and sulphur compound are 'bonded together and form a monolithic r structure, andfapplying a thin layer of the sulphur compound-to exposed surfaces of said structure by painting the compound in a molten condition upon such surfaces.

-9. The method of making structures composed of a compound of intimatelyA mixed sulphur and finely divided carbonac'eous ma- `terial which comprises appropriately confining a mass of aggregate materialv composed of suitably sized lumps of the sulphur compound at approximatelyA atmospheric f temperature, fillingV the voids throughout the mass of the aggregate material With't e sulphur compound in a. molten condition,

and permitting such molten sulphur compound to' solidify in situ in the mass of aggregate material whereby the aggregate andl molten materials form a monolithic structure composed throughout of a substantially homogeneous mass of intimately mixed sulphur and carbonaceous materiali l 10. The method of making receptacles for corrosive liquors andthe like which comprises appropriately confining a mass of aggregate material composed of a compound of Aintimately mixed sulphurand'finely divided carbonaceous material at approximately atmospheric temperature, filling the voids t throughout the mass of aggregate material with a olten compound of intimately mixed sulphur and finely divided carbonaceous material, and permitting suchl molten sulphur compound to solidify inl situ in the mass of aggregate material whereby the ag,-v gregate and molten materials ultimatelyl form a monolithic structurecomposed throughout of a substantiallyhomogeneous mass of intimately mixed' sulphur and carbonaceous material. V

`ll; As .a new article of manufacture, a

structure composedat least in part of a com- -pound of intimately 'mixed 'sulphur and finely divided carbonaceous material and comprising a mass of aggregate material.

with the individual lumps thereof united and bonded togetherby the compound of sulphur and carbonaceous material. i

12.'As a new article of manufacture, a structure composed at least in part of a com- .pound of intimately mixed sulphur and finely divided carbonaceous material` and comprisingl a; massi of aggregate material `with the spaces between the individual lumps thereof filled with and .the `lumps united and bonded together by the compoundof sulphur and carbonaceous maf.

terial. y

- 13. As a new article of manufacture, a structure composed at least in part of a 

